#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:55:54 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179431 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/28/4332873.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4332873
loop_
_publ_author_name
'Sugiura, Tetsuya'
'Yoshikawa, Hirofumi'
'Awaga, Kunio'
_publ_section_title
;
 1D Helical Polymeric Chain with a Pseudo-53Screw Axis Formed by
 Cuprophilicity. Synthesis and Crystal Structure of Copper(I) Pivalate
;
_journal_issue                   19
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7584
_journal_page_last               7586
_journal_paper_doi               10.1021/ic060989b
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C25 H45 Cu5 O10'
_chemical_formula_weight         823.31
_chemical_name_common            Copperpivalate
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.067(4)
_cell_angle_beta                 95.692(6)
_cell_angle_gamma                101.207(7)
_cell_formula_units_Z            2
_cell_length_a                   6.353(2)
_cell_length_b                   13.136(5)
_cell_length_c                   21.035(8)
_cell_measurement_reflns_used    4172
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.1680
_cell_volume                     1710.7(11)
_computing_molecular_graphics    'ORTEP 3 for windows'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0678
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            13903
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    3.103
_exptl_absorpt_correction_T_max  0.5757
_exptl_absorpt_correction_T_min  0.5757
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod-like
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.946
_refine_diff_density_min         -1.044
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         7516
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.1133
_refine_ls_R_factor_gt           0.0885
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0476P)²+28.5212P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2188
_refine_ls_wR_factor_ref         0.2323
_reflns_number_gt                5568
_reflns_number_total             7516
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060989bsup1.cif
_cod_data_source_block           Cupivalate
_cod_original_cell_volume        1710.6(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4332873
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cu1 Cu -0.3297(2) 0.31904(10) 0.26051(6) 0.0384(3) Uani 1 1 d .
Cu2 Cu -0.2294(2) 0.13467(9) 0.20367(6) 0.0355(3) Uani 1 1 d .
Cu3 Cu 0.0451(2) 0.24228(9) 0.31207(6) 0.0351(3) Uani 1 1 d .
Cu4 Cu 0.2057(2) 0.24395(9) 0.19023(6) 0.0353(3) Uani 1 1 d .
Cu5 Cu 0.3868(2) 0.12713(10) 0.28543(6) 0.0359(3) Uani 1 1 d .
O1 O -0.3122(13) 0.3551(6) 0.1770(4) 0.0477(19) Uani 1 1 d .
C1 C -0.2823(16) 0.3030(8) 0.1292(5) 0.035(2) Uani 1 1 d .
C2 C -0.2809(18) 0.3510(9) 0.0647(5) 0.040(2) Uani 1 1 d .
C3 C -0.068(2) 0.3403(13) 0.0392(6) 0.069(4) Uani 1 1 d .
H1 H -0.0613 0.3697 -0.0018 0.104 Uiso 1 1 calc R
H2 H -0.0608 0.2681 0.0351 0.104 Uiso 1 1 calc R
H3 H 0.0506 0.3764 0.0685 0.104 Uiso 1 1 calc R
C4 C -0.304(3) 0.4635(10) 0.0709(6) 0.065(4) Uani 1 1 d .
H4 H -0.3018 0.4925 0.0297 0.098 Uiso 1 1 calc R
H5 H -0.1871 0.5021 0.0998 0.098 Uiso 1 1 calc R
H6 H -0.4387 0.4670 0.0873 0.098 Uiso 1 1 calc R
C5 C -0.471(2) 0.2860(10) 0.0208(6) 0.053(3) Uani 1 1 d .
H7 H -0.4750 0.3134 -0.0209 0.079 Uiso 1 1 calc R
H8 H -0.6035 0.2889 0.0384 0.079 Uiso 1 1 calc R
H9 H -0.4531 0.2152 0.0175 0.079 Uiso 1 1 calc R
O2 O -0.2569(13) 0.2098(6) 0.1314(3) 0.0453(18) Uani 1 1 d .
O3 O -0.2222(11) 0.0266(5) 0.2570(3) 0.0374(16) Uani 1 1 d .
C6 C -0.1436(15) 0.0305(7) 0.3145(5) 0.032(2) Uani 1 1 d .
C7 C -0.1843(16) -0.0675(7) 0.3505(5) 0.035(2) Uani 1 1 d .
C8 C -0.4272(18) -0.0975(10) 0.3543(7) 0.058(3) Uani 1 1 d .
H10 H -0.4582 -0.1596 0.3772 0.088 Uiso 1 1 calc R
H11 H -0.5013 -0.1095 0.3119 0.088 Uiso 1 1 calc R
H12 H -0.4746 -0.0421 0.3763 0.088 Uiso 1 1 calc R
C9 C -0.070(3) -0.0525(11) 0.4175(6) 0.072(4) Uani 1 1 d .
H13 H -0.1002 -0.1164 0.4387 0.107 Uiso 1 1 calc R
H14 H -0.1189 0.0009 0.4408 0.107 Uiso 1 1 calc R
H15 H 0.0831 -0.0325 0.4156 0.107 Uiso 1 1 calc R
C10 C -0.111(2) -0.1530(9) 0.3125(7) 0.063(4) Uani 1 1 d .
H16 H -0.1356 -0.2161 0.3347 0.094 Uiso 1 1 calc R
H17 H 0.0402 -0.1324 0.3081 0.094 Uiso 1 1 calc R
H18 H -0.1912 -0.1641 0.2709 0.094 Uiso 1 1 calc R
O4 O -0.0402(12) 0.1130(5) 0.3445(3) 0.0412(17) Uani 1 1 d .
O5 O 0.1372(12) 0.3842(5) 0.3071(4) 0.0434(18) Uani 1 1 d .
C11 C 0.2169(16) 0.4310(7) 0.2604(5) 0.035(2) Uani 1 1 d .
C12 C 0.2764(19) 0.5494(8) 0.2675(6) 0.046(3) Uani 1 1 d .
C13 C 0.394(3) 0.5935(11) 0.2113(9) 0.093(6) Uani 1 1 d .
H19 H 0.4302 0.6680 0.2170 0.139 Uiso 1 1 calc R
H20 H 0.3015 0.5738 0.1721 0.139 Uiso 1 1 calc R
H21 H 0.5232 0.5665 0.2097 0.139 Uiso 1 1 calc R
C14 C 0.436(4) 0.5757(13) 0.3268(9) 0.113(8) Uani 1 1 d .
H22 H 0.4791 0.6499 0.3334 0.170 Uiso 1 1 calc R
H23 H 0.5606 0.5463 0.3215 0.170 Uiso 1 1 calc R
H24 H 0.3699 0.5478 0.3632 0.170 Uiso 1 1 calc R
C15 C 0.073(3) 0.5877(12) 0.2728(14) 0.143(11) Uani 1 1 d .
H25 H 0.1050 0.6623 0.2774 0.214 Uiso 1 1 calc R
H26 H 0.0083 0.5601 0.3094 0.214 Uiso 1 1 calc R
H27 H -0.0245 0.5656 0.2349 0.214 Uiso 1 1 calc R
O6 O 0.2484(11) 0.3864(5) 0.2091(4) 0.0407(17) Uani 1 1 d .
O7 O 0.1624(13) 0.1168(5) 0.1461(3) 0.0443(18) Uani 1 1 d .
C16 C 0.2125(15) 0.0337(8) 0.1650(5) 0.033(2) Uani 1 1 d .
C17 C 0.1595(18) -0.0614(8) 0.1180(5) 0.039(2) Uani 1 1 d .
C18 C 0.246(3) -0.1504(10) 0.1465(6) 0.066(4) Uani 1 1 d .
H28 H 0.1778 -0.1699 0.1842 0.099 Uiso 1 1 calc R
H29 H 0.3994 -0.1295 0.1578 0.099 Uiso 1 1 calc R
H30 H 0.2176 -0.2087 0.1158 0.099 Uiso 1 1 calc R
C19 C 0.263(2) -0.0295(10) 0.0571(6) 0.060(3) Uani 1 1 d .
H31 H 0.2058 0.0273 0.0397 0.090 Uiso 1 1 calc R
H32 H 0.2321 -0.0874 0.0261 0.090 Uiso 1 1 calc R
H33 H 0.4167 -0.0084 0.0671 0.090 Uiso 1 1 calc R
C20 C -0.085(2) -0.0901(10) 0.1044(6) 0.058(3) Uani 1 1 d .
H34 H -0.1464 -0.1105 0.1431 0.086 Uiso 1 1 calc R
H35 H -0.1242 -0.1467 0.0726 0.086 Uiso 1 1 calc R
H36 H -0.1392 -0.0312 0.0891 0.086 Uiso 1 1 calc R
O8 O 0.3027(13) 0.0262(6) 0.2200(3) 0.0438(18) Uani 1 1 d .
O9 O 0.4576(12) 0.1879(6) 0.3677(3) 0.0433(17) Uani 1 1 d .
C21 C -0.4209(15) 0.2736(8) 0.3856(4) 0.033(2) Uani 1 1 d .
O10 O -0.3211(12) 0.3346(6) 0.3488(4) 0.0446(18) Uani 1 1 d .
C22 C -0.3934(17) 0.3043(9) 0.4568(4) 0.041(2) Uani 1 1 d .
C23 C -0.618(2) 0.3050(12) 0.4768(6) 0.064(4) Uani 1 1 d .
H37 H -0.7077 0.2373 0.4677 0.096 Uiso 1 1 calc R
H38 H -0.6809 0.3552 0.4535 0.096 Uiso 1 1 calc R
H39 H -0.6065 0.3229 0.5218 0.096 Uiso 1 1 calc R
C24 C -0.248(2) 0.4073(12) 0.4702(6) 0.078(5) Uani 1 1 d .
H40 H -0.1078 0.4039 0.4576 0.118 Uiso 1 1 calc R
H41 H -0.2343 0.4260 0.5152 0.118 Uiso 1 1 calc R
H42 H -0.3060 0.4585 0.4466 0.118 Uiso 1 1 calc R
C25 C -0.301(2) 0.2193(13) 0.4916(6) 0.069(4) Uani 1 1 d .
H43 H -0.1596 0.2183 0.4794 0.103 Uiso 1 1 calc R
H44 H -0.3937 0.1530 0.4801 0.103 Uiso 1 1 calc R
H45 H -0.2916 0.2335 0.5370 0.103 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Cu1 O10 159.2(3) . .
O1 Cu1 Cu2 79.0(2) . .
O10 Cu1 Cu2 119.5(2) . .
O1 Cu1 Cu3 112.0(2) . .
O10 Cu1 Cu3 74.1(3) . .
Cu2 Cu1 Cu3 59.83(4) . .
O1 Cu1 Cu5 118.9(3) . 1_455
O10 Cu1 Cu5 79.8(2) . 1_455
Cu2 Cu1 Cu5 65.21(5) . 1_455
Cu3 Cu1 Cu5 91.20(5) . 1_455
O3 Cu2 O2 162.5(3) . .
O3 Cu2 Cu1 115.7(2) . .
O2 Cu2 Cu1 80.2(2) . .
O3 Cu2 Cu3 79.6(2) . .
O2 Cu2 Cu3 116.3(3) . .
Cu1 Cu2 Cu3 60.44(5) . .
O3 Cu2 Cu4 110.3(2) . .
O2 Cu2 Cu4 75.1(3) . .
Cu1 Cu2 Cu4 90.88(5) . .
Cu3 Cu2 Cu4 59.14(5) . .
O5 Cu3 O4 161.7(3) . .
O5 Cu3 Cu4 80.6(2) . .
O4 Cu3 Cu4 116.5(2) . .
O5 Cu3 Cu2 116.4(3) . .
O4 Cu3 Cu2 79.7(2) . .
Cu4 Cu3 Cu2 60.93(5) . .
O5 Cu3 Cu1 74.2(3) . .
O4 Cu3 Cu1 110.0(2) . .
Cu4 Cu3 Cu1 91.52(5) . .
Cu2 Cu3 Cu1 59.73(5) . .
O5 Cu3 Cu5 111.6(2) . .
O4 Cu3 Cu5 75.3(2) . .
Cu4 Cu3 Cu5 58.76(4) . .
Cu2 Cu3 Cu5 90.30(5) . .
Cu1 Cu3 Cu5 146.59(6) . .
O7 Cu4 O6 162.2(3) . .
O7 Cu4 Cu3 115.6(3) . .
O6 Cu4 Cu3 80.5(2) . .
O7 Cu4 Cu5 80.0(2) . .
O6 Cu4 Cu5 115.8(3) . .
Cu3 Cu4 Cu5 62.57(5) . .
O7 Cu4 Cu2 72.1(3) . .
O6 Cu4 Cu2 113.4(2) . .
Cu3 Cu4 Cu2 59.93(4) . .
Cu5 Cu4 Cu2 91.93(5) . .
O8 Cu5 O9 160.0(3) . .
O8 Cu5 Cu4 79.9(2) . .
O9 Cu5 Cu4 117.7(2) . .
O8 Cu5 Cu1 118.5(3) . 1_655
O9 Cu5 Cu1 79.4(2) . 1_655
Cu4 Cu5 Cu1 65.84(5) . 1_655
O8 Cu5 Cu3 113.6(2) . .
O9 Cu5 Cu3 72.6(3) . .
Cu4 Cu5 Cu3 58.67(5) . .
Cu1 Cu5 Cu3 90.61(5) 1_655 .
C1 O1 Cu1 130.1(7) . .
O1 C1 O2 122.9(9) . .
O1 C1 C2 119.5(9) . .
O2 C1 C2 117.6(9) . .
C1 C2 C4 110.8(9) . .
C1 C2 C3 106.9(9) . .
C4 C2 C3 111.9(11) . .
C1 C2 C5 106.7(9) . .
C4 C2 C5 110.8(10) . .
C3 C2 C5 109.6(10) . .
C1 O2 Cu2 127.4(7) . .
C6 O3 Cu2 128.5(6) . .
O3 C6 O4 123.5(9) . .
O3 C6 C7 118.2(8) . .
O4 C6 C7 118.2(9) . .
C9 C7 C6 112.2(9) . .
C9 C7 C10 110.6(11) . .
C6 C7 C10 108.1(9) . .
C9 C7 C8 108.8(10) . .
C6 C7 C8 107.5(8) . .
C10 C7 C8 109.5(10) . .
C6 O4 Cu3 127.7(7) . .
C11 O5 Cu3 127.1(7) . .
O6 C11 O5 124.6(9) . .
O6 C11 C12 118.4(9) . .
O5 C11 C12 117.0(9) . .
C15 C12 C14 113.2(16) . .
C15 C12 C11 107.2(10) . .
C14 C12 C11 106.2(11) . .
C15 C12 C13 112.4(14) . .
C14 C12 C13 106.7(13) . .
C11 C12 C13 110.9(10) . .
C11 O6 Cu4 127.0(7) . .
C16 O7 Cu4 128.3(7) . .
O8 C16 O7 123.1(9) . .
O8 C16 C17 119.3(9) . .
O7 C16 C17 117.6(8) . .
C18 C17 C20 110.4(11) . .
C18 C17 C16 110.4(9) . .
C20 C17 C16 107.2(9) . .
C18 C17 C19 110.8(10) . .
C20 C17 C19 110.9(10) . .
C16 C17 C19 107.1(9) . .
C16 O8 Cu5 128.6(7) . .
C21 O9 Cu5 128.5(7) 1_655 .
O9 C21 O10 124.5(9) 1_455 .
O9 C21 C22 117.0(9) 1_455 .
O10 C21 C22 118.5(9) . .
C21 O10 Cu1 127.8(7) . .
C24 C22 C21 110.6(9) . .
C24 C22 C23 111.7(11) . .
C21 C22 C23 107.4(9) . .
C24 C22 C25 111.1(11) . .
C21 C22 C25 107.2(9) . .
C23 C22 C25 108.7(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.844(8) .
Cu1 O10 1.855(7) .
Cu1 Cu2 2.871(2) .
Cu1 Cu3 2.891(2) .
Cu1 Cu5 2.897(2) 1_455
Cu2 O3 1.846(7) .
Cu2 O2 1.853(7) .
Cu2 Cu3 2.8738(19) .
Cu2 Cu4 2.902(2) .
Cu3 O5 1.852(7) .
Cu3 O4 1.854(7) .
Cu3 Cu4 2.850(2) .
Cu3 Cu5 2.9619(19) .
Cu4 O7 1.841(7) .
Cu4 O6 1.860(7) .
Cu4 Cu5 2.8531(19) .
Cu5 O8 1.840(7) .
Cu5 O9 1.854(7) .
Cu5 Cu1 2.897(2) 1_655
O1 C1 1.247(12) .
C1 O2 1.268(12) .
C1 C2 1.516(13) .
C2 C4 1.516(16) .
C2 C3 1.530(16) .
C2 C5 1.536(16) .
O3 C6 1.256(11) .
C6 O4 1.264(11) .
C6 C7 1.509(13) .
C7 C9 1.509(15) .
C7 C10 1.526(15) .
C7 C8 1.527(14) .
O5 C11 1.274(12) .
C11 O6 1.261(12) .
C11 C12 1.525(14) .
C12 C15 1.485(19) .
C12 C14 1.51(2) .
C12 C13 1.532(19) .
O7 C16 1.262(12) .
C16 O8 1.256(11) .
C16 C17 1.527(13) .
C17 C18 1.506(16) .
C17 C20 1.522(16) .
C17 C19 1.534(16) .
O9 C21 1.257(11) 1_655
C21 O9 1.257(11) 1_455
C21 O10 1.259(11) .
C21 C22 1.521(12) .
C22 C24 1.483(16) .
C22 C23 1.529(16) .
C22 C25 1.535(17) .
